Search results for: Photoluminescence Spectroscopy (PL) and Field Effect Scanning electron microscopy (FESEM)

Authors: Gabi N. Nehme, Saeed Ghalambor

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The use of titanium fluoride and iron fluoride (TiF3/FeF3) catalysts in combination with polutetrafluoroethylene (PTFE) in plain zinc dialkyldithiophosphate (ZDDP) oil is important for the study of engine tribocomponents and is increasingly a strategy to improve the formation of tribofilm and to provide low friction and excellent wear protection in reduced phosphorus plain ZDDP oil. The influence of surface roughness and the concentration of TiF3/FeF3/PTFE were investigated using bearing steel samples dipped in lubricant solution @100°C for two different heating time durations. This paper addresses the effects of water drop contact angle using different surface finishes after treating them with different lubricant combination. The calculated water drop contact angles were analyzed using Design of Experiment software (DOE) and it was determined that a 0.05 μm Ra surface roughness would provide an excellent TiF3/FeF3/PTFE coating for antiwear resistance as reflected in the scanning electron microscopy (SEM) images and the tribological testing under extreme pressure conditions. Both friction and wear performance depend greatly on the PTFE/and catalysts in plain ZDDP oil with 0.05% phosphorous and on the surface finish of bearing steel. The friction and wear reducing effects, which was observed in the tribological tests, indicated a better micro lubrication effect of the 0.05 μm Ra surface roughness treated at 100°C for 24 hours when compared to the 0.1 μm Ra surface roughness with the same treatment.

Keywords: scanning electron microscopy, ZDDP, catalysts, PTFE, friction, wear

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Authors: S. Kerakra, S. Bouhelal, M. Poncot

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The aim of this study is to give a comprehensive overview of the effect of short hollow and solid recycled polyethylene terephthalate (PET) fibers in different breaking tenacities reinforced isotactic polypropylene (iPP) composites on the mechanical and morphological properties. Composites of iPP/3, 7and 10 wt% of solid and hollow recycled PET fibers were prepared by batched melt mixing in a Brabender. The incorporation of solid recycled-PET fibers in isotactic polypropylene increase Young’s modulus of iPP relatively, meanwhile it increased proportionally with hollow fibers content. An improvement of the storage modulus, and a shift up in glass transition temperatures of hollow fibers/iPP composites was determined by DMA results. The morphology of composites was determined by scanning electron microscope (SEM) and optical polarized microscopy (OM) showing a good dispersion of the hollow fibers. Also, their flexible aspect (folding, bending) was observed. But, one weak interaction between the polymer/fibers phases was shown. Polymers can be effectively reinforced with short hollow recycled PET fibers due to their characteristics like recyclability, lightweight and the flexible aspect, which allows the absorbance of the energy of a striker with a minimum damage of the matrix. Aiming to improve the affinity matrix–recycled hollow PET fibers, it is suggested the addition of compatibilizers, as maleic anhydride.

Keywords: isotactic polypropylene, hollow recycled PET fibers, solid recycled-PET fibers, composites, short fiber, scanning electron microscope

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Authors: Vaibhav Budhiraja, Chandra Mouli Pandey

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The ultrasonic synthesis of nanostructured conducting copolymer is an effective technique to synthesize polymer with desired chemical properties. This tailored nanostructure, shows tremendous improvement in sensitivity and stability to detect a variety of analytes. The present work reports ultrasonically synthesized nanostructured conducting poly(o-phenylenediamine)-co-poly(1-naphthylamine) (POPD-co-PNA). The synthesized material has been characterized using Fourier transform infrared spectroscopy (FTIR), ultraviolet-visible spectroscopy, transmission electron microscopy, X-ray diffraction and cyclic voltammetry. FTIR spectroscopy confirmed random copolymerization, while UV-visible studies reveal the variation in polaronic states upon copolymerization. High crystallinity was achieved via ultrasonic synthesis which was confirmed by X-ray diffraction, and the controlled morphology of the nanostructures was confirmed by transmission electron microscopy analysis. Cyclic voltammetry shows that POPD-co-PNA has rather high electrochemical activity. This behavior was explained on the basis of variable orientations adopted by the conducting polymer chains. The synthesized material was electrophoretically deposited at onto indium tin oxide coated glass substrate which is used as cathode and parallel platinum plate as the counter electrode. The fabricated bioelectrode was further used for detection of glucose by crosslinking of glucose oxidase in the PODP-co-PNA film. The bioelectrode shows a surface-controlled electrode reaction with the electron transfer coefficient (α) of 0.72, charge transfer rate constant (ks) of 21.77 s⁻¹ and diffusion coefficient 7.354 × 10⁻¹⁵ cm²s⁻¹.

Keywords: conducting, electrophoretic, glucose, poly (o-phenylenediamine), poly (1-naphthylamine), ultrasonic

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Authors: Reim A. Almotiri, Manal M. Alkhamisi

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Ternary nanocomposites based on hydroxyapatite (HAP) and alumina (Al2O3) were embedded through graphene oxide (GO) nanosheets to be investigated for medical applications. The composition of the preparations has been confirmed by X-ray photoelectron spectroscopy, energy-dispersive X-ray analysis, and Fourier-Transform infrared spectroscopy. Scanning and transmission electron microscopy have shown the typical morphologies of the components of the nanocomposites with hydroxyapatite nanorods reaching an average diameter of 22.26±2 nm and an average length of 69.56±19.25 nm in the ternary nanocomposites. The ternary nanocomposite has a microhardness of 5.8±0.1 GPa and a higher average roughness of 6.5 nm compared to pure HAP preparation with an average roughness of 2.7 nm. All preparations have shown an acceptable cytotoxicity profile with a percent osteoblasts cell viability of 98.6±1.3% after culturing with the ternary nanocomposite. The TNC has also shown the highest antibacterial activity compared to preparations of each of its constituents and their nanocomposites, with a zone of inhibition’s diameter of 14.1±0.8 mm and 13.6±0.6 mm against Staphylococcus aureus and Escherichia coli, respectively, compared to no zone of inhibition for the pure hydroxyapatite preparation.

Keywords: hydroxypatite, cytotoxicity, nanocomposites, X-ray analysis

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Authors: Byungsik Moon

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Electron beam inspection (EBI) has played an important role in detecting defects during the Fab process. The study focused on capturing buried Cu metal voids for 5nm technology nodes in Qualcomm Snapdragon mass production. This paper illustrates a case study where Cu metal voids can be detected without side effects with optimized EBI scanning conditions. The voids were buried in the VIA and not detected effectively by bright field inspection. EBI showed higher detectability, about 10 times that of bright fields, and a lower landing energy of EBI can avoid film damage. A comparison of detectability between EBI and bright field inspection was performed, and TEM confirmed voids that were detected by EBI. Therefore, a much higher detectability of buried Cu metal voids can be achieved without causing film damage.

Keywords: electron beam inspection, EBI, landing energy, Cu metal voids, bright field inspection

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Authors: Ainouna Bouziane

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The ability of Electron Tomography to recover the 3D structure of catalysts, with spatial resolution in the subnanometer scale, has been widely explored and reviewed in the last decades. A variety of experimental techniques, based either on Transmission Electron Microscopy (TEM) or Scanning Transmission Electron Microscopy (STEM) have been used to reveal different features of nanostructured catalysts in 3D, but High Angle Annular Dark Field imaging in STEM mode (HAADF-STEM) stands out as the most frequently used, given its chemical sensitivity and avoidance of imaging artifacts related to diffraction phenomena when dealing with crystalline materials. In this regard, our group has developed a methodology that combines image denoising by undecimated wavelet transforms (UWT) with automated, advanced segmentation procedures and parameter selection methods using CS-TVM (Compressed Sensing-total variation minimization) algorithms to reveal more reliable quantitative information out of the 3D characterization studies. However, evaluating the accuracy of the magnitudes estimated from the segmented volumes is also an important issue that has not been properly addressed yet, because a perfectly known reference is needed. The problem particularly complicates in the case of multicomponent material systems. To tackle this key question, we have developed a methodology that incorporates volume reconstruction/segmentation methods. In particular, we have established an approach to evaluate, in quantitative terms, the accuracy of TVM reconstructions, which considers the influence of relevant experimental parameters like the range of tilt angles, image noise level or object orientation. The approach is based on the analysis of material-realistic, 3D phantoms, which include the most relevant features of the system under analysis.

Keywords: electron tomography, supported catalysts, nanometrology, error assessment

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Authors: G. Nyongombe, Guy L. Kabongo, B. M. Mothudi, M. S. Dhlamini

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A series of Transition Metals Oxides (TMOs) doped graphene were synthesized and successfully used as supercapacitor electrode materials. The as-synthesized materials exhibited exceptional electrochemical properties owing to the combined properties of its constituents; high surface area and good conductivity were achieved. Several analytical characterization techniques were employed to investigate the morphology, crystal structure atomic arrangement and elemental chemical state in the materials for which scanning electron microscopy (SEM), X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS) were conducted, respectively. Moreover, the electrochemical properties of the as-synthesized materials were examined by performing cyclic voltammetry (CV), galvanostatic charge-discharge (GCD) and electrochemical impedance spectroscopy (EIS) measurements. Furthermore, the effect of doping concentration on the interlayer distance of the graphene materials and the charge transfer resistance are investigated and correlated to the exceptional current density which was multiplied by a factor of ~80 after TMOs doping in graphene. Finally, the resulting high capacitance obtained confirms the contribution of grapheme exceptional electronic conductivity and large surface area on the electrode materials. Such good-performing electrode materials are highly promising for supercapacitors and other energy storage devices.

Keywords: energy density, graphene, supercapacitors, TMOs

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Authors: Bharat Kumar, Deepak Kumar, Vijay Chaudhry

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Zirconium alloys are used as core components of nuclear reactors due to their high wear resistance, good corrosion properties, and good mechanical stability at high temperatures. Water flows inside the pressure tube through fuel claddings, which produces vibration of these core components and results in the wear of some components. Some components are subjected to the environment of coolant water containing LiOH which results in the corrosion of these components. The present work simulates some of these conditions to determine the failure mechanisms under these conditions and the effect of various parameters on them. Friction and wear experiments were performed varying the surrounding environment (room temperature, high temperature, and water submerged), duration, frequency, and displacement amplitude. Electrochemical corrosion experiments were performed by varying the concentration of LiOH in water. The worn and corroded surfaces were analyzed using scanning electron microscopy (SEM) to analyze the wear and corrosion mechanism and energy dispersive x-ray spectroscopy (EDS) and Raman spectroscopy to analyze the tribo-oxide layer formed during the wear and oxide layer formed during the corrosion. Wear increases with frequency and amplitude, and corrosion increases with LiOH concentration in water.

Keywords: zirconium alloys, wear, oxide layer, corrosion, EIS, linear polarization

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Authors: Djamil Guettiche, Ahmed Mekki, Tighilt Fatma-Zohra, Rachid Mahmoud

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The aim of this study was to synthesize and characterize conducting polymer composites of polypyrrole and graphene, including pristine and surface-treated graphene (PPy/GO, PPy/rGO, and PPy/rGO-ArCOOH), for use as sensitive elements in a homemade chemiresistive module for on-line detection of nitrogen oxides vapors. The chemiresistive module was prepared, characterized, and evaluated for performance. Structural and morphological characterizations of the composite were carried out using FTIR, Raman spectroscopy, and XRD analyses. After exposure to NO and NO₂ gases in both static and dynamic modes, the sensitivity, selectivity, limit of detection, and response time of the sensor were determined at ambient temperature. The resulting sensor showed high sensitivity, selectivity, and reversibility, with a low limit of detection of 1 ppm. A composite of polypyrrole and graphene functionalized with aryl 4-carboxy benzene diazonium salt was synthesized and characterized using FTIR, scanning electron microscopy, transmission electron microscopy, UV-visible, and X-ray diffraction. The PPy-rGOArCOOH composite exhibited a good electrical resistance response to NO₂ at room temperature and showed enhanced NO₂-sensing properties compared to PPy-rGO thin films. The selectivity and stability of the NO₂ sensor based on the PPy/rGO-ArCOOH nanocomposite were also investigated.

Keywords: conducting polymers, surface treated graphene, diazonium salt, polypyrrole, Nitrogen oxide sensing

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Authors: Suraj D. Khadka, Priyantha W. Jayawickrama

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In search of a sustainable construction material, geopolymer has been investigated for past decades to evaluate its advantage over conventional products. Synthesis of geopolymer requires a source of aluminosilicate mixed with sodium hydroxide and sodium silicate at different proportions to maintain a Si/Al molar ratio of 1-3 and Na/Al molar ratio of unity. A comprehensive geopolymer study was performed with Metakaolin and Class C Fly ash as primary aluminosilicate sources. Synthesized geopolymer was analyzed for time-dependent viscosity, setting period and strength at varying initial moisture content, curing temperature and humidity. Different concentration of Ca(OH)₂ and CaSO₄.2H₂O were added to vary the amount of calcium contained in synthesized geopolymer. Influence of calcium content in unconfined compressive strength behavior of geopolymer were analyzed. Finally, Scanning Electron Microscopy-Energy Dispersive Spectroscopy (SEM-EDS) was performed to investigate the hardened product. It was observed that fly ash based geopolymer had shortened setting time and faster increase in viscosity as compared to geopolymer synthesized from metakaolin. This was primarily attributed to higher calcium content resulting in formation of calcium silicate hydrates (CSH). SEM-EDS was performed to verify the presence of CSH phases. Spectral analysis of geopolymer prepared by addition of Ca(OH)₂ and CaSO₄.2H₂O indicated higher CSH phases at higher concentration. It was observed that lower concentration of added calcium favored strength gain in geopolymer. However, at higher calcium concentration, decrease in strength was observed. Strength variation was also observed with humidity at initial curing condition. At 100% humidity, geopolymer with added calcium presented higher strength compared to samples cured at ambient humidity condition (40%). Reduction in strength in these samples at lower humidity was primarily attributed to reduction in moisture content in specimen due to the formation of CSH phases and loss of moisture through evaporation. For low calcium content geopolymers, with increase in temperature, gain in strength was observed with maximum strength observed at 200 ˚C. However, samples with higher calcium content demonstrated severe cracking resulting in low strength at elevated temperatures.

Keywords: calcium silicate hydrates, geopolymer, humidity, Scanning Electron Microscopy-Energy Dispersive Spectroscopy, unconfined compressive strength

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Authors: Sweta Iyer, Nemeshwaree Behary, Jinping Guan, Guoqiang Chen, Vincent Nierstrasz

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Flavin mononucleotide widely known as 'FMN' is a biobased resource derived from riboflavin. The isoalloxazine ring present in the FMN molecule attributes the photoluminescence phenomenon, whereas FMN molecule in the presence of bacterial luciferase enzyme and co-factors such as NADH, long chain aldehyde leads to bioluminescence reaction. In this study, the FMN molecule was treated on cellulosic textile using chromojet technique and the photoluminescence property was characterized using spectroscopy technique. Further, the FMN was used as a substrate along with enzymes and co-factors to treat the non-woven textile, and the bioluminescence property was explored using luminometer equipment. The investigation revealed photoluminescence property on cellulosic textile, and the emission peak was observed at a wavelength around 530 nm with an average corrected spectral intensity of 10×106 CPS/Microamps. In addition, the measurement of nonwoven textile using bioluminescence reaction system exhibited light intensity measured in the form of relative light units (RLU). The study enabled to explore the use of FMN as both photoluminescent and bioluminescent textile. Further investigation would require for stability study of the same to provide an eco-efficient approach to obtain luminescent textile.

Keywords: flavin mononucleotide, photoluminescence, bioluminescence, luminescent textile

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Authors: Hyunho Shin, Jaekwang Jung, Jeongho Park, Sungwon Hwang

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For the application of graphene quantum dots (GQDs) to optoelectronic nanodevices, it is of critical importance to understand the mechanisms which result in novel phenomena of their light absorption/emission. The optical transitions are known to be available up to ~6 eV in GQDs, especially useful for ultraviolet (UV) photodetectors (PDs). Here, we present size-dependent shape/edge-state variations of GQDs and visible photoluminescence (PL) showing anomalous size dependencies. With varying the average size (da) of GQDs from 5 to 35 nm, the peak energy of the absorption spectra monotonically decreases, while that of the visible PL spectra unusually shows nonmonotonic behaviors having a minimum at diameter ∼17 nm. The PL behaviors can be attributed to the novel feature of GQDs, that is, the circular-to-polygonal-shape and corresponding edge-state variations of GQDs at diameter ∼17 nm as the GQD size increases, as demonstrated by high resolution transmission electron microscopy. We believe that such a comprehensive scheme in designing device architecture and the structural formulation of GQDs provides a device for practical realization of environmentally benign, high performance flexible devices in the future.

Keywords: graphene, quantum dot, size, photoluminescence

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Authors: Leonnel Mhuka

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Background: The field of photonics has witnessed substantial growth, with an increasing demand for miniaturized and high-performance optical components. Microstructured optical waveguides have gained significant attention due to their ability to confine and manipulate light at the subwavelength scale. Conventional fabrication methods, however, face limitations in achieving intricate and customizable waveguide structures. Two-photon polymerization (TPP) emerges as a promising additive manufacturing technique, enabling the fabrication of complex 3D microstructures with submicron resolution. Objectives: This experiment aimed to utilize two-photon polymerization to fabricate microstructured optical waveguides with precise control over geometry and dimensions. The objective was to demonstrate the feasibility of TPP as an additive manufacturing method for producing functional waveguide devices with enhanced performance. Methods: A femtosecond laser system operating at a wavelength of 800 nm was employed for two-photon polymerization. A custom-designed CAD model of the microstructured waveguide was converted into G-code, which guided the laser focus through a photosensitive polymer material. The waveguide structures were fabricated using a layer-by-layer approach, with each layer formed by localized polymerization induced by non-linear absorption of the laser light. Characterization of the fabricated waveguides included optical microscopy, scanning electron microscopy, and optical transmission measurements. The optical properties, such as mode confinement and propagation losses, were evaluated to assess the performance of the additive manufactured waveguides. Conclusion: The experiment successfully demonstrated the additive manufacturing of microstructured optical waveguides using two-photon polymerization. Optical microscopy and scanning electron microscopy revealed the intricate 3D structures with submicron resolution. The measured optical transmission indicated efficient light propagation through the fabricated waveguides. The waveguides exhibited well-defined mode confinement and relatively low propagation losses, showcasing the potential of TPP-based additive manufacturing for photonics applications. The experiment highlighted the advantages of TPP in achieving high-resolution, customized, and functional microstructured optical waveguides. Conclusion: his experiment substantiates the viability of two-photon polymerization as an innovative additive manufacturing technique for producing complex microstructured optical waveguides. The successful fabrication and characterization of these waveguides open doors to further advancements in the field of photonics, enabling the development of high-performance integrated optical devices for various applications

Keywords: Additive Manufacturing, Microstructured Optical Waveguides, Two-Photon Polymerization, Photonics Applications

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Authors: Qiao Yushuang, Shao Longyi

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This paper presents the result of plasmid assay of inhalable particulates PM10 and PM2.5 that were collected during the period of the 11th Hanyuan temple fair of ancestor worship in Kaifeng City. By use of a high-resolution Field Emission Scanning Electron Microscopy (FESEM) and image analysis (IA) technology, the morphological characteristics and Particle Size Distribution (PSD) of each were analyzed and the Bioreactivity of PM10 was evaluated by using plasmid DNA assay. The result shows that, as the dominant component of the samples taken in the urban area of Kaifeng City, the mineral particles, compared with the other components including the soot aggregates, coal ash, and unidentified particles, have a much greater amount and volume. The mineral particles exhibited a decentralized quantity - size distribution, whose presence could be available among the particles sizing 2.5μm or smaller. In contrast, the volume-size distribution of mineral particles is scattered in a relatively narrow range of between1μm and 2.5μm. According to the plasmid assay the TD50 (toxic dose of PM causing 50% of plasmid damage, expressed in μg/ml) of water-soluble PM10 and whole fraction of Kaifeng airborne PM10 was measured respectively at 220-208μg/ml and 300-400μg/ml versus 160μg/ml and 190μg/ml for PM2.5. It can be seen that the whole fraction of airborne particles caused more oxidative damage than the water-soluble fractions, and the PM2.5 has a greater oxidative capacity than the PM10.

Keywords: inhalable particulates (PM10 and PM2.5), morphological features, bioreactivity, Kaifeng

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Authors: Olga Długosz, Jolanta Pulit-Prociak, Marcin Banach

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The paper presents a process to obtain glutathione-modified titanium oxide nanoparticles. The processes were carried out in a microwave radiation field. The influence of the molar ratio of glutathione to titanium oxide and the effect of the fold of NaOH vs. stoichiometric amount on the size of the formed TiO₂ nanoparticles was determined. The physicochemical properties of the obtained products were evaluated using dynamic light scattering (DLS), transmission electron microscope- energy-dispersive X-ray spectroscopy (TEM-EDS), low-temperature nitrogen adsorption method (BET), X-Ray Diffraction (XRD) and Fourier-transform infrared spectroscopy (FTIR) microscopy methods. The size of TiO₂ nanoparticles was characterized from 30 to 336 nm. The release of titanium ions from the prepared products was evaluated. These studies were carried out using different media in which the powders were incubated for a specific time. These were water, SBF and Ringer's solution. The release of titanium ions from modified products is weaker compared to unmodified titanium oxide nanoparticles. The reduced release of titanium ions may allow the use of such modified materials as substances in drug delivery systems.

Keywords: titanium dioxide, nanoparticles, drug carrier, glutathione

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Authors: Olga Długosz, Jolanta Pulit-Prociak, Marcin Banach

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The paper presents a process to obtain glutathione-modified titanium oxide nanoparticles. The processes were carried out in a microwave radiation field. The influence of the molar ratio of glutathione to titanium oxide and the effect of the fold of NaOH vs. stoichiometric amount on the size of the formed TiO₂ nanoparticles was determined. The physicochemical properties of the obtained products were evaluated using dynamic light scattering (DLS), transmission electron microscope- energy-dispersive X-ray spectroscopy (TEM-EDS), low-temperature nitrogen adsorption method (BET), X-Ray Diffraction (XRD), and Fourier-transform infrared spectroscopy (FTIR) microscopy methods. The size of TiO₂ nanoparticles was characterized from 30 to 336 nm. The release of titanium ions from the prepared products was evaluated. These studies were carried out using different media in which the powders were incubated for a specific time. These were: water, SBF, and Ringer's solution. The release of titanium ions from modified products is weaker compared to unmodified titanium oxide nanoparticles. The reduced release of titanium ions may allow the use of such modified materials as substances in drug delivery systems.

Keywords: titanium dioxide, nanoparticles, drug carrier, glutathione

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Authors: Raghvendra Singh Yadav, Ivo Kuřitka

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In this report, we studied the impact of Gd3+ substitution on structural, magnetic and electrical properties of CoFe2O4 nanoparticles synthesized by sonochemical method. X-ray diffraction pattern confirmed the formation of cubic spinel structure at low concentration of Gd3+ ions, however, GdFeO3 additional phase was observed at higher concentration of Gd3+ ions. Raman and Fourier Transform Infrared spectroscopy study also confirmed cubic spinel structure of Gd3+ substituted CoFe2O4 nanoparticles. The field emission scanning electron microscopy study revealed that Gd3+ substituted CoFe2O4 nanoparticles were in the range of 5-20 nm. The magnetic properties of Gd3+ substituted CoFe2O4 nanoparticles were investigated by using vibrating sample magnetometer. The variation in saturation magnetization, coercivity and remanent magnetization with Gd3+ concentration in CoFe2O4 nanoparticles was observed. The variation of real and imaginary part of dielectric constant, tan δ, and AC conductivity were studied at room temperature.

Keywords: spinel ferrites, nanoparticles, sonochemical method, magnetic properties

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Authors: Parvathy Anitha, Nilesh J. Vasa, M. S. Ramachandra Rao

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ZnO is a semiconducting material with a direct wide band gap of 3.37 eV and a large exciton binding energy of 60 meV at room temperature. Microspheres with high sphericity and symmetry exhibit unique functionalities which makes them excellent omnidirectional optical resonators. Hence there is an advent interest in fabrication of single crystalline semiconductor microspheres especially magnetic ZnO microspheres, as ZnO is a promising material for semiconductor device applications. Also, ZnO is non-toxic and biocompatible, implying it is a potential material for biomedical applications. Room temperature Photoluminescence (PL) spectra of the fabricated ZnO microspheres were measured, at an excitation wavelength of 325 nm. The ultraviolet (UV) luminescence observed is attributed to the room-temperature free exciton related near-band-edge (NBE) emission in ZnO. Besides the NBE luminescence, weak and broad visible luminescence (~560nm) was also observed. This broad emission band in the visible range is associated with oxygen vacancies related to structural defects. In transition metal (TM) ion-doped ZnO, 3d levels emissions of TM ions will modify the inherent characteristic emissions of ZnO. A micron-sized ZnO crystal has generally a wurtzite structure with a natural hexagonal cross section, which will serve as a WGM (whispering gallery mode) lasing micro cavity due to its high refractive index (~2.2). But hexagonal cavities suffers more optical loss at their corners in comparison to spherical structures; hence spheres may be a better candidate to achieve effective light confinement. In our study, highly smooth spherical shaped micro particles with different diameters ranging from ~4 to 6 μm were grown on different substrates. SEM (Scanning Electron Microscopy) and AFM (Atomic Force Microscopy) images show the presence of uniform smooth surfaced spheres. Raman scattering measurements from the fabricated samples at 488 nm light excitation provide convincing supports for the wurtzite structure of the prepared ZnO microspheres. WGM lasing studies from TM-doped ZnO microparticles are in progress.

Keywords: laser ablation, microcavity, photoluminescence, ZnO microsphere

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Authors: Chetna Tyagi. G. B. V. S. Lakshmi, Ambuj Tripathi, D. K. Avasthi

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Graphene oxide provides a good host matrix for preparing nanocomposites due to the different functional groups attached to its edges and planes. Being biocompatible, it is used in therapeutic applications. As enzyme-based biosensor requires complicated enzyme purification procedure, high fabrication cost and special storage conditions, we need enzyme-less biosensors for use even in a harsh environment like high temperature, varying pH, etc. In this work, we have prepared both enzyme-based and enzyme-less graphene oxide-based biosensors for glucose detection using glucose-oxidase as enzyme and gold nanoparticles, respectively. These samples were characterized using X-ray diffraction, UV-visible spectroscopy, scanning electron microscopy, and transmission electron microscopy to confirm the successful synthesis of the working electrodes. Electrochemical measurements were performed for both the working electrodes using a 3-electrode electrochemical cell. Cyclic voltammetry curves showed the homogeneous transfer of electron on the electrodes in the scan range between -0.2V to 0.6V. The sensing measurements were performed using differential pulse voltammetry for the glucose concentration varying from 0.01 mM to 20 mM, and sensing was improved towards glucose in the presence of gold nanoparticles. Gold nanoparticles in graphene oxide nanocomposite played an important role in sensing glucose in the absence of enzyme, glucose oxidase, as evident from these measurements. The selectivity was tested by measuring the current response of the working electrode towards glucose in the presence of the other common interfering agents like cholesterol, ascorbic acid, citric acid, and urea. The enzyme-less working electrode also showed storage stability for up to 15 weeks, making it a suitable glucose biosensor.

Keywords: electrochemical, enzyme-less, glucose, gold nanoparticles, graphene oxide, nanocomposite

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Authors: Afiqah Shafify Amran, Siti Aisyah Shamsudin, Nurul Yuziana Mohd Yusof

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Cadmium Sulphide (CdS) from group II-IV quantum dots with good optical properties was successfully synthesized by using the simple colloidal method. Capping them with ligand Polyethylinamine (PEI) alters the surface defect of CdS while, thioglycolic acid (TGA) was added to the reaction as a stabilizer. Due to their cytotoxicity, we decided to conjugate them with the protein cage nanoparticles. In this research, we used capsid of Cowpea Chlorotic Mottle Virus (CCMV) to package the CdS because they have the potential to serve in drug delivery, cell targeting and imaging. Adding Sodium Hydroxide (NaOH) changes the pH of the systems hence the isoelectric charge is adjusted. We have characterized and studied the morphology and the optical properties of CdS and CdS-CCMV by transmitted electron microscopic (TEM), UV-Vis spectroscopy, photoluminescence spectroscopy, UV lamp and Fourier transform infrared spectroscopy (FTIR), respectively. The results obtained suggest that the protein cage nanoparticles do not affect the optical properties of CdS.

Keywords: cadmium sulphide, cowpea chlorotic mottle virus, protein cage nanoparticles, quantum dots

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Authors: Asiful Hossain Seikh, Mohammad Asif Alam, Ubair Abdus Samad, Jabair A. Mohammed, S. M. Al-Zahrani, El-Sayed M. Sherif

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In this current investigation, aliphatic amine-cured diglycidyl ether of bisphenol-A (DGEBA) based epoxy coating was mixed with certain weight % hardener polyaminoamide (1:2) and was coated on carbon steel panels with and without 1% nano crystalline Al powder. The corrosion behavior of the coated samples were investigated by exposing them in the salt spray chamber, for 500 hours. According to ASTM-B-117, the bath was kept at 35 °C and 5% NaCl containing mist was sprayed at 1.3 bars pressure. Composition of coatings was confirmed using Fourier-transform infrared spectroscopy (FTIR). Electrochemical characterization of the coated samples was also performed using potentiodynamic polarization technique and electrochemical impedance spectroscopy (EIS) technique. All the experiments were done in 3.5% NaCl solution. The nano Al coated sample shows good corrosion resistance property compared to bare Al sample. In fact after salt spray exposure no pitting or local damage was observed for nano coated sample and the coating gloss was negligibly affected. The surface morphology of coated and corroded samples was studied using scanning electron microscopy (SEM).

Keywords: epoxy, nano aluminium, potentiodynamic polarization, salt spray, electrochemical impedence spectroscopy

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Authors: Marcia Silva, Jayme Kolarik, Brennon Garthwait, William Lee, Hai-Feng Zhang

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Adsorption of lead by a natural porous material was studied to establish a baseline for the removal of heavy metals from drinking and waste water. Samples were examined under different conditions such as solution pH, solution concentration, solution temperature, and exposure time. New materials with potentially enhanced adsorption properties were developed by functionalizing the surface of the natural porous material to fabricate graphene based coated and sulfide based treated porous material. The functionalized materials were characterized with Fourier Transform Infrared Spectroscopy (FTIR), Raman, Thermogravimetric Analysis (TGA) and Scanning Electron Microscopy (SEM) and Energy Dispersive Spectroscopy (EDS) techniques. Solution pH effect on removal efficiency has been investigated in acidic (pH = 4), neutral (pH = 6) and basic (pH = 10) pH levels. All adsorbent materials showed highest adsorption capacities at neutral pH levels. Batch experiment was employed to assess the efficacy for the removal of lead with the sorption kinetics and the adsorption isotherms being determined for the natural and treated porous materials. The addition of graphene-based and sulfide-based materials increased the lead removal capacity of the natural clean porous material. Theoretical calculations confirmed pseudo-second order model as kinetic mechanism for lead adsorption for all adsorbents.

Keywords: heavy metals, ion exchange, adsorption, water remediation

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Authors: H. K. G. K. D. K. Hapuhinna, R. D. Gunaratne, H. M. J. C. Pitawala

Abstract:

Hydroxyapatite is a bioceramic which can be used for applications in orthopedics and dentistry due to its structural similarity with the mineral phase of mammalian bones and teeth. In this study, it was synthesized, chemically changing natural Eppawala chloroapatite mineral as a value-added product. Sol-gel approach and solid state sintering were used to synthesize products using diluted nitric acid, ethanol and calcium hydroxide under different conditions. Synthesized Eppawala hydroxyapatite powder was characterized using X-ray Fluorescence (XRF), X-ray Powder Diffraction (XRD), Fourier-transform Infrared Spectroscopy (FTIR), Scanning Electron Microscopy (SEM), Thermogravimetric Analysis (TGA) and Differential Scanning Calorimetry (DSC) in order to find out its composition, crystallinity, presence of functional groups, bonding type, surface morphology, microstructural features, and thermal dependence and stability, respectively. The XRD results reflected the formation of a hexagonal crystal structure of hydroxyapatite. Elementary composition and microstructural features of products were discussed based on the XRF and SEM results of the synthesized hydroxyapatite powder. TGA and DSC results of synthesized products showed high thermal stability and good material stability in nature. Also, FTIR spectroscopy results confirmed the formation of hydroxyapatite from apatite via the presence of hydroxyl groups. Those results coincided with the FTIR results of mammalian bones including human bones. The study concludes that there is a possibility of producing hydroxyapatite using commercially available Eppawala chloroapatite in Sri Lanka.

Keywords: dentistry, Eppawala chlorapatite, hydroxyapatite, orthopedics

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Authors: Davoud Dorranian, Hajar Sadeghi, Elmira Solati

Abstract:

Carbon nanostructures in various forms were synthesized using pulsed laser ablation of a graphite target in different liquid environment. The beam of a Q-switched Nd:YAG laser of 1064-nm wavelength at 7-ns pulse width is employed to irradiate the solid target in water, acetone, alcohol, and cetyltrimethylammonium bromide (CTAB). Then the effect of the liquid environment on the characteristic of carbon nanostructures produced by laser ablation was investigated. The optical properties of the carbon nanostructures were examined at room temperature by UV–Vis-NIR spectrophotometer. The crystalline structure of the carbon nanostructures was analyzed by X-ray diffraction (XRD). The morphology of samples was investigated by field emission scanning electron microscope (FE-SEM). Transmission electron microscope (TEM) was employed to investigate the form of carbon nanostructures. Raman spectroscopy was used to determine the quality of carbon nanostructures. Results show that different carbon nanostructures such as nanoparticles and few-layer graphene were formed in various liquid environments. The UV-Vis-NIR absorption spectra of samples reveal that the intensity of absorption peak of nanoparticles in alcohol is higher than the other liquid environments due to the larger number of nanoparticles in this environment. The red shift of the absorption peak of the sample in acetone confirms that produced carbon nanoparticles in this liquid are averagely larger than the other medium. The difference in the intensity and shape of the absorption peak indicated the effect of the liquid environment in producing the nanoparticles. The XRD pattern of the sample in water indicates an amorphous structure due to existence the graphene sheets. X-ray diffraction pattern shows that the degree of crystallinity of sample produced in CTAB is higher than the other liquid environments. Transmission electron microscopy images reveal that the generated carbon materials in water are graphene sheet and in the other liquid environments are graphene sheet and spherical nanostructures. According to the TEM images, we have the larger amount of carbon nanoparticles in the alcohol environment. FE-SEM micrographs indicate that in this liquids sheet like structures are formed however in acetone, produced sheets are adhered and these layers overlap with each other. According to the FE-SEM micrographs, the surface morphology of the sample in CTAB was coarser than that without surfactant. From Raman spectra, it can be concluded the distinct shape, width, and position of the graphene peaks and corresponding graphite source.

Keywords: carbon nanostructures, graphene, pulsed laser ablation, graphite

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Authors: Bahaa Fawwaz‬‏

Abstract:

The study was conducted on a papyrus housed at the Museum of Islamic Art in Cairo, Egypt. This papyrus was inscribed with black ink. Twelve fungal species were isolated and identified. Five types of fungi were ultimately identified to complete the study. The isolated fungi were then incubated for three months after the aging procedure. This study investigates the in-vitro growth inhibition of Aspergillus niger, Aspergillus flavus, Penicillium chrysogenum, Trichoderma longibrachiatum Rifai, and Paecilomyces variotii on papyrus. The hyphal growth was observed using the environmental scanning electron microscope (ESEM). Natural oils, such as lavender oil, lemongrass oil, and rosemary oil, were used. The impact of these natural oils on the newly aged papyrus was assessed using scanning electron microscopy and color analysis to identify the most effective oils for inhibiting fungus growth.

Keywords: conservation, papyrus, fungi, growth, environmental, essential oils

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Authors: Mauricio Gómez, Esmeralda López, Ian Becar, Jaime Pizarro, Paula A. Zapata

Abstract:

A biodegradable material is developed with adsorptive capacity for metals ion for intended use in mining tailings mitigating the environmental impact with economic retribution, two types of fibers were elaborated by electrospinning: (1) a cellulose acetate (CA) matrix and (2) a cellulose acetate (CA)/chitosan (CH) matrix evaluating the effect of CH in CA on its physicochemical properties. Through diffuse reflectance infrared fourier transform spectroscopy (DRIFTS) the incorporation of chitosan in the matrix was identified, observing the band of the amino group at 1500 - 1600 [cm-1]. By scanning electron microscopy (SEM), Hg porosimetry, and CO2 isotherm at 273 [K], the intrafiber microporosity and interfiber macroporosity were identified, with an increase in the distribution of macropores for CA/CH fibers. In the tensile test, CH into the matrix produces a more ductile and tenacious behavior, where the % elongation at break increased by 33% with the other parameters constant. Thermal analysis by differential scanning calorimetry (DSC) and Thermogravimetric Analysis (TGA) showed that the incorporation of chitosan produces higher retention of water molecules due to the functional groups (amino groups (- NH3)), but there is a decrease in the specific heat and thermoplastic properties of the matrix since the glass transition temperature and softening temperature disappear. The effect of the optimum pH for CA and CA/CH fibers were studied in a batch system. In the adsorption kinetic study, the best isotherm model adapted to the experimental results corresponds to the Sips model and the kinetics corresponds to pseudo-second order

Keywords: environmental materials, wastewater treatment, electrospun fibers, biopolymers (cellulose acetate/chitosan), metals recovery

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Authors: Saba Didarataee, Abbas Ali Khodadadi, Yadollah Mortazavi, Fatemeh Mousavi

Abstract:

Photocatalytic water splitting is one of the most attractive alternative methods for hydrogen evolution. A variety of nanoparticle engineering techniques were introduced to improve the activity of semiconductor photocatalysts. Among these methods, heterojunction formation is an appealing method due to its ability to effectively preventing electron-hole recombination and improving photocatalytic activity. Reaching an optimal ratio of the two target semiconductors for the formation of heterojunctions is still an open question. Considering environmental issues as well as the cost and availability, ZnS and ZnO are frequently studied as potential choices. In this study, first, the ZnS nanoparticle was synthesized in a hydrothermal process; the formation of ZnS nanorods with a diameter of 14-30 nm was confirmed by field emission scanning electron microscope (FESEM). Then two different methods, partial oxidation and chemical precipitation were employed to construct ZnS/ZnO core-shell heterojunction. X-ray diffraction (XRD), BET, and diffuse reflectance spectroscopy (DRS) analysis were carried out to determine crystallite phase, surface area, and bandgap of photocatalysts. Furthermore, the temperature of oxidation was specified by a temperature programmed oxidation (TPO) and was fixed at 510℃, at which mild oxidation occurred. The bandgap was calculated by the Kubelka-Munk method and decreased by increasing oxide content from 3.53 (pure ZnS) to 3.18 (pure ZnO). The optimal samples were determined by testing the photocatalytic activity of hydrogen evolution in a quartz photoreactor with side irradiation of UVC lamps with a wavelength of 254 nm. In both procedures, it was observed that the photocatalytic activity of the ZnS/ZnO composite was sensibly higher than the pure ZnS and ZnO, which is attributed to forming a type-II heterostructure. The best ratio of oxide to sulfide was 0.24 and 0.37 in partial oxidation and chemical precipitation, respectively. The highest hydrogen evolution was 1081 µmol/gr.h, gained from partial oxidizing of ZnS nanoparticles at 510℃ for 30 minutes.

Keywords: heterostructure, hydrogen, partial oxidation, photocatalyst, water splitting, ZnS

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Authors: Babak Azari, Afshin Pourahmad, Babak Sadeghi, Masuod Mokhtari

Abstract:

In this work, Equisetnm arvense plant extract was used for preparing amorphous SiO₂. For preparing of SiO₂/zeolitic imidazolate framework-8 (ZIF-8) nanocomposite by solvothermal method, the synthesized SiO₂ was added to the synthesis mixture ZIF-8. The nanocomposite was characterized using a range of techniques. The photocatalytic activity of SiO₂/ZIF-8 was investigated systematically by degrading crystal violet as a cationic dye under Ultraviolet light irradiation. Among synthesized samples (SiO₂, ZIF-8 and SiO₂/ZIF-8), the SiO₂/ZIF-8 exhibited the highest photocatalytic activity and improved stability compared to pure SiO₂ and ZIF-8. As evidenced by Scanning Electron Microscopy and Transmission electron microscopy images, ZIF-8 particles without aggregation are located over SiO₂. The SiO₂ not only provides structured support for ZIF-8 but also prevents the aggregation of ZIF-8 Metal-organic framework in comparison to the isolated ZIF-8. The superior activity of this photocatalyst was attributed to the synergistic effects from SiO₂ owing to (I) an electron acceptor (from ZIF-8) and an electron donor (to O₂ molecules), (II) preventing recombination of electron-hole in ZIF-8, and (III) maximum interfacial contact ZIF-8 with the SiO₂ surface without aggregation or prevent the accumulation of ZIF-8. The results demonstrate that holes (h+) and •O₂- are primary reactive species involved in the photocatalytic oxidation process. Moreover, the SiO₂/ZIF-8 photocatalyst did not show any obvious loss of photocatalytic activity during five-cycle tests, which indicates that the heterostructured photocatalyst was highly stable and could be used repeatedly.

Keywords: nano, zeolit, potocatalist, nanocomposite

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Authors: Fernando G. Torres, Donna M. Ebenstein, Monica Merino

Abstract:

Most fish are covered by a protective external armour. The characteristics of these armours depend on the individual elements that form them, such as scales, scutes or dermal plates. In this work, we assess the properties of two different types of protective elements: scales from A. gigas and dermal plates from P. pardalis. A. Gigas and P. Pardalis are two Amazonian fish with a rather prehistoric aspect. They have large scales and dermal plates that form two different types of protective body armours. Although both scales and dermal plates are formed by collagen and hydroxyapatite, their structures display remarkable differences. The structure and composition of the samples were assessed by means of X-ray diffraction (XRD), Fourier Transform Infrared spectroscopy (FTIR) and Differential Scanning Calorimetry (DSC). Morphology studies were carried out using a Scanning Electron Microscopy (SEM). Nanoindentation tests were performed to measure the reduced moduli in A. gigas scales and P. pardalis plates. The similarities and differences between scales and dermal plates are discussed based on the experimental results. Both protective armours are designed to be lightweight, flexible and tough. A. Gigas scales are are light laminated composites, while P. pardalis dermal plates show a sandwich like structure with dense outer layers and a porous inner matrix. It seems that the armour of P. pardalis is more suited for a bottom-dwelling fish and allows for protection against predators. The scales from A. Gigas are more adapted to give protection to a swimming fish. The information obtained from these studies is also important for the development of bioinspired nanocomposites, with potential applications in the biomedical field.

Keywords: pterygoplichthys pardalis, dermal plates arapaima gigas, fish scales

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Authors: Burcu Kiren, Alattin CAkan, Nezihe Ayas

Abstract:

Hydrogen will be arguably the best fuel in the future as it is the most abundant element in the universe. Hydrogen, as a fuel, is notably environmentally benign, sustainable and has high energy content compared to other sources of energy. It can be generated from both conventional and renewable sources. The hydrolysis reaction of metal hydrides provides an option for hydrogen production in the presence of a catalyst. In this study, Ni/dolomite catalyst was synthesized by the wet impregnation method for hydrogen production by hydrolysis reaction of sodium borohydride (NaBH4). Besides, the synthesized catalysts characterizations were examined by means of thermogravimetric analysis (TGA), Fourier-transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), Brunauer –Emmett – Teller (BET) and scanning electron microscopy (SEM). The influence of reaction temperature (25-75 °C), reaction time (15-60 min.), amount of catalyst (50-250 mg) and active metal loading ratio (20,30,40 wt.%) were investigated. The catalyst prepared with 30 wt.% Ni was noted as the most suitable catalyst, achieving of 35.18% H₂ and hydrogen production rate of 19.23 mL/gcat.min at 25 °C at reaction conditions of 5 mL of 0.25 M NaOH and 100 mg NaBH₄, 100 mg Ni/dolomite.

Keywords: sodium borohydride, hydrolysis, catalyst, Ni/dolomite, hydrogen

Procedia PDF Downloads 166